EP2692691A1 - Magnesit- und Hydromagnesit-Herstellungsverfahren - Google Patents

Magnesit- und Hydromagnesit-Herstellungsverfahren Download PDF

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EP2692691A1
EP2692691A1 EP12305943.8A EP12305943A EP2692691A1 EP 2692691 A1 EP2692691 A1 EP 2692691A1 EP 12305943 A EP12305943 A EP 12305943A EP 2692691 A1 EP2692691 A1 EP 2692691A1
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comprised
medium
magnesite
hydromagnesite
brucite
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French (fr)
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German Montez Hernandez
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Centre National de la Recherche Scientifique CNRS
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/24Magnesium carbonates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/88Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM

Definitions

  • the present invention relates to a magnesite and hydromagnesite preparation process.
  • reaction path for the MgO-H 2 O-CO 2 slurry at ambient temperatures and at atmospheric CO 2 partial pressure is of both geological interest and practical significance.
  • the knowledge of the reaction path with this slurry would lead to a better understanding of the low temperature alteration or weathering of mafic and ultramafic rocks.
  • exact knowledge of the reaction path in this slurry is important to the performance assessment of geological repositories for nuclear waste where mineral periclase MgO and brucite Mg(OH) 2 have been proposed as engineered barriers ( Xiong, Y.; Lord, A. S. Appl. Geochem. 2008, 23, 1634 ).
  • MgO-H 2 O-CO 2 or Mg(OH) 2 -H 2 O-CO 2 slurries a significant number of hydrated and basic (or hydroxylated) carbonates (e.g. nesquehontite, lansfordite, artinite, hydromagnesite, dypingite, pokrosvskite, etc.) can be formed at ambient temperature and at moderate CO 2 pressure ( ⁇ 55 bar) ( Hanchen, M.; Prigiobbe, V.; Baciocchi, R.; Mazzotti, M. Chem. Eng. Sci. 2008, 63, 1012 , Langmuir, D. The Journal of Geology 1965, 73, 730 ; Oh, K.
  • the minimal reported temperature for the production of magnesite is about 60-100°C, its formation also requiring the presence of elevated CO 2 pressure ( Deelman, J. C. Chemie Der Erde-Geochemistry 2001, 61, 224 ; Usdowski, E. Naturwissenschaften 1989, 76, 374 ).
  • the magnesite is obtained by transformation of a pre-existent hydroxylated Mg-carbonate such as the hydromagnesite ( Sandengen, K.; Josang, L. O.; Kaasa, B. Ind. Eng. Chem. Res. 2008, 47, 1002 , Stevula, L.; Petrovic, J.; Kubranova, M. Chemicke Zvesti 1978, 32, 441 ).
  • This transition can be very slow; for example, below 150°C and at moderate pressures, its duration is often in the order of days.
  • Higher temperatures, high salinity, high CO 2 pressure, low magnesium concentration (in closed apparatus) and the use of organic additives (ex. monoethylene glycol) are known to accelerate the hydromagnesite-to-magnesite transformation ( Sandengen, K.; Josang, L. O.; Kaasa, B. Ind. Eng. Chem. Res. 2008, 47, 1002 ; Zhang, L. Sandia National Laboratories, Albuquerque, USA 2000 , Technical Report SAN099-19465).
  • Reported transformation times are comprised between 2h at 200°C in a solution saturated with NaCl, and over 100 days at 110°C at lower salinity in a closed apparatus.
  • Magnesite formation without an apparent initial or intermediate hydromagnesite presence has also been reported under high CO 2 pressures (100-150 bar) and at high temperatures (150-180°C), for experiments coupling the dissolution of Mg-silicates with carbonate precipitation ( Giammar D. E.; Bruant Jr., R. G.; Peters, C. A. Chem. Geol. 2005, 217, 257 , Bearat, H.; Mckelvy, M. J.; Chizmeshya, A. V.
  • One of the aims of the present invention is to provide a simple method of carbonation of brucite for the preparation hydromagnesite and magnesite.
  • Another aim of the invention is to provide a preparation process of magnesite and hydromagnesite in two steps at low temperature and low CO 2 pressure.
  • the present invention relates to the use of brucite and a CO 2 source in a medium having a pH higher than 13, in particular 13.5, and containing a strong base, at a temperature comprised from about 15°C to about 40°C, in particular from about 16°C to about 20°C, during a t 1 time comprised from about 2h to about 25h, for the preparation of magnesite and/or hydromagnesite.
  • the inventors have surprisingly found that the strong alkalinity of the medium accelerate the brucite carbonation by increasing the concentration of carbonate ions.
  • a strong base such as NaOH increases the trapping of CO 2 forming Na 2 CO 3 which is spontaneously dissociated into Na + and CO 3 - , that is to say a fast availability and a high concentration of carbonate ions that will react with brucite.
  • the brucite has the following formula: Mg(OH) 2 .and can be from synthetic or natural origin.
  • brucite is from synthetic origin and can be prepared by methods well known from a man skilled in the art.
  • the CO 2 source can be pure or concentrated CO 2 gas, i.e. CO 2 gas containing a small proportion of SO x or NO x , or a stream containing a low concentration of CO 2 gas such as flue gas or industrial off-gas or a mixture of CO 2 gas with an inert gas such as, for example, nitrogen, argon or air.
  • the reaction of brucite with CO 2 is named a carbonation reaction.
  • the medium containing brucite and CO 2 must be highly alkaline, i.e. higher than 13, in particular 13.5.
  • medium an aqueous medium, in particular water, advantageously high-purity water.
  • the medium contains slurry of brucite-H 2 O-CO 2 and the strong base.
  • strong base is meant a base giving a pH of the medium higher than 13, in particular 13.5.
  • the temperature of the medium is comprised from about 15°C to about 40°C, in particular it is the room temperature, i.e. from 16° to 20°C.
  • reaction medium necessitates to be heated to reach the temperature which is expensive for a production at industrial scale.
  • the magnesite and hydromagnesite have the respective following formulae: Mg(CO 3 ) and Mg 5 (CO 3 ) 4 (OH) 2 .4H 2 O.
  • the carbonation reaction must be carried out at a controlled time between 2h to 25h depending of the final required product (magnesite or hydromagnesite).
  • the present invention relates to the use of brucite and a CO 2 source in a medium having a pH higher than 13, in particular 13.5, as defined above, wherein said base is selected from the group consisting of NaOH, KOH, LiOH and RbOH, preferentially NaOH, preferably at a molar ratio NaOH/brucite comprised from 1 to 3, in particular 2.
  • the base plays a catalytic role by accelerating the brucite carbonation as already stated above.
  • the number of molar equivalents of the base must be at least the one of brucite but no more than 3. Above 3, the molar concentration of the base does not improve the speed of the reaction or the yield of magnesite of hydromagnesite obtained.
  • the base is NaOH because of its availability and is preferentially 2M NaOH.
  • the present invention relates to the use of brucite and a CO 2 source in a medium having a pH higher than 13, in particular 13.5, as defined above, wherein the CO 2 source in the medium is at a initial pressure comprised from about 40bar to about 60bar, in particular 50bar.
  • initial pressure is meant the pressure of the CO 2 source when it is introduced into the alkaline medium.
  • the pressure used for the carbonation reaction is an anisobaric pressure that means that the pressure is not constant during the carbonation reaction, i.e. variable between the beginning and the end of the process. As the CO 2 source is consumed, CO 2 pressure drops in the system, i.e. the apparatus containing the reaction medium.
  • an isobaric pressure can be used, i.e. at a constant CO 2 pressure during the reaction, by introducing CO 2 as soon as it is consumed.
  • the present invention relates to the use of brucite and a CO 2 source in a medium having a pH higher than 13, in particular 13.5, the CO 2 source in the medium being at a initial pressure comprised from about 40bar to about 60bar, in particular 50bar, as defined above, wherein said t 1 time is comprised from 23h to about 25h, in particular 24h, enabling the formation of an intermediate comprising a dypingite precipitate in the medium.
  • the inventors have surprisingly found that the control of the t 1 time allows to monitor the intermediates formed in the reaction, a t 1 time comprised from 23 to 25h, in particular 24h, allowing to form a precipitate of dypingite, the structure of which is the following: (Mg 5 (CO 3 ) 4 (OH) 2 .5H 2 O). Said dypingite is under the form of platy-compacted aggregates.
  • the present invention relates to the use of brucite and a CO 2 source in a medium having a pH higher than 13, in particular 13.5, the CO 2 source in the medium being at a initial pressure comprised from about 40bar to about 60bar, in particular 50bar, said t 1 time being comprised from 23h to about 25h, in particular 24h, enabling the formation of an intermediate comprising a dypingite precipitate in the medium, as defined above, wherein said medium containing the dypingite is further heated, after said t 1 time, at a temperature comprised from about 80°C to about 100°C, in particular 90°C, during a t 2 time comprised from about 20 to about 30 h, in particular 24h, for the preparation of magnesite, comprising less than 2% of eitelite.
  • the inventors have surprisingly found that heating the dypingite precipitate at about 80°C to about 100°C, in particular 90°C during about 20 to about 30 h, in particular 24h, leads to the precipitation of the magnesite in the medium.
  • This heating step is named heat-ageing step.
  • magnesite in a complete time of 48h, can be formed from brucite if the medium contains a strong base such as NaOH, KOH, LiOH and RbOH, in particular NaOH.
  • the magnesite obtained is constituted of rhombohedral single crystals ( ⁇ 2 ⁇ m) of magnesite, eventually comprising eitelite that is a marker of the process of the invention in a proportion less than 2% by weight compared with magnesite.
  • the present invention relates to the use of brucite and a CO 2 source in a medium having a pH higher than 13, in particular 13.5, the CO 2 source in the medium being at a initial pressure comprised from about 40bar to about 60bar, in particular 50bar, as defined above, wherein said t 1 time is comprised from 2h to about 4h, in particular 3h, enabling the formation of an intermediate comprising a mixture of residual brucite and a hydrated Mg carbonate in the medium.
  • control of the t 1 time allows to control the intermediates formed in the reaction, a t 1 time comprised from 2 to 4h, in particular 3h, allowing to form an intermediate comprising a mixture of the optionally residual brucite and a hydrated Mg carbonate.
  • residual brucite means that a small quantity of brucite that has not yet reacted can be present in the medium that will be further transformed into hydromagnesite during the heat-ageing step.
  • hydrated Mg carbonate is meant a mixture of compounds of the dypingite type, i.e. of various mineral phases. and/or an amorphous hydrated Mg carbonate that forms a suspension in the medium.
  • the introduction of brucite and the strong base is carried out at room temperature and thus an initial temperature (t i ) of about 26°C is observed in the medium before introducing CO 2 , said medium reaching 37 ⁇ 1°C until the complete or almost complete formation of said intermediate.
  • the present invention relates to the use of brucite and a CO 2 source in a medium having a pH higher than 13, in particular 13.5, the CO 2 source in the medium being at a initial pressure comprised from about 40bar to about 60bar, in particular 50bar, said t 1 time being comprised from 2h to about 4h, in particular 3h, enabling the formation of an intermediate comprising a mixture of residual brucite and of hydrated Mg carbonate in the medium, as defined above, wherein said medium is further heated, after said t 1 time, at a temperature comprised from about 80°C to about 100°C, in particular 90°C during a t 2 time comprised from about 1 to about 3h, in particular 2h, for the preparation of hydromagnesite, comprising less than 2% of brucite.
  • the inventors have surprisingly found that heating the mixture of residual brucite and of hydrated Mg carbonate at about 80°C to about 100°C, in particular 90°C, during a t 2 time comprised from about 1 to about 3h, in particular 2h, leads to the precipitation of the hydromagnesite in the medium.
  • Hydromagnesite is obtained under a precipitate form and has the following structure: Mg 5 (CO 3 ) 4 (OH) 2 .4H 2 O.
  • This heating step is named heat-ageing step.
  • hydromagnesite in a complete time of 5h, can be formed from brucite if the medium contains a strong base such as NaOH, KOH, LiOH and RbOH, in particular NaOH.
  • the present invention relates to a process of preparation of magnesite and/or hydromagnesite comprising a step of contacting brucite and a CO 2 source in a medium having a pH higher than 13, in particular 13.5, and containing a strong base, at a temperature comprised from about 15°C to about 40°C, in particular from about 16°C to about 20°C, during a t 1 time comprised from about 2h to about 25h.
  • the step of contacting brucite and a CO 2 source in a medium having a pH higher than 13, in particular 13.5, and containing a strong base is carried out at 16°C.
  • the step of contacting brucite and a CO 2 source in a medium having a pH higher than 13, in particular 13.5, and containing a strong base is carried out at 17°C.
  • the step of contacting brucite and a CO 2 source in a medium having a pH higher than 13, in particular 13.5, and containing a strong base is carried out at 18°C.
  • the step of contacting brucite and a CO 2 source in a medium having a pH higher than 13, in particular 13.5, and containing a strong base is carried out at 19°C.
  • the step of contacting brucite and a CO 2 source in a medium having a pH higher than 13, in particular 13.5, and containing a strong base is carried out at 20°C.
  • the present invention relates to a process of preparation of magnesite and/or hydromagnesite, as defined above, wherein said base is NaOH, preferably at a molar ratio NaOH/brucite comprised from 1 to 3, in particular 2.
  • the present invention relates to a process of preparation of magnesite and/or hydromagnesite, as defined above, wherein the CO 2 source in the medium is at an initial pressure comprised from about 40 bar to about 60 bar, in particular 50 bar.
  • initial pressure is meant the pressure of the CO 2 source when it is introduced into the alkaline medium.
  • the pressure used for the carbonation reaction is an anisobaric pressure that means that the pressure is not constant during the carbonation reaction, i.e. variable between the beginning and the end of the process. As the CO 2 source is consumed, CO 2 pressure drops in the system, i.e. the apparatus containing the reaction medium.
  • an isobaric pressure can be used, i.e. at a constant CO 2 pressure during the reaction, by introducing CO 2 as soon as it is consumed.
  • the present invention relates to a process of preparation of magnesite and/or hydromagnesite, wherein the CO 2 source in the medium is at an initial pressure comprised from about 40 bar to about 60 bar, in particular 50bar, as defined above, wherein said t 1 time is comprised from 23h to about 25h, in particular 24h, to obtain an intermediate comprising a dypingite precipitate in the medium.
  • the strong base in particular NaOH, plays a catalytic role, i.e. it accelerates the brucite carbonation by a temporary increase of carbonate ion concentration
  • the present invention relates to a process of preparation of magnesite and/or hydromagnesite, wherein the CO 2 source in the medium is at an initial pressure comprised from about 40 bar to about 60 bar, in particular 50bar, wherein said t 1 time is comprised from 23h to about 25h, in particular 24h, to obtain an intermediate comprising a dypingite precipitate in the medium, as defined above, comprising a further step of heating the medium containing the dypingite, after said t 1 time, at a temperature comprised from about 80°C to about 100°C, in particular 90°C, during a t 2 time comprised from about 20 to about 30 h, in particular 24h to obtain magnesite.
  • the strong base in particular NaOH, not only plays a catalytic role but also favors the magnesite formation during the heat-ageing step.
  • the present invention relates to one of the above process of preparation of magnesite comprising the following steps:
  • the precipitation of magnesite at low temperature is kinetically inhibited by a preferential precipitation of hydrated and/or hydroxylated Mg-carbonates (e.g. nesquehontite, lansfordite, artinite, hydromagnesite, dypingite, pokrosvskite%), possibly due to high hydration character of Mg 2+ ions in solution. Based on this assumption, the formation of magnesite at ambient temperature is virtually impossible.
  • Mg-carbonates e.g. nesquehontite, lansfordite, artinite, hydromagnesite, dypingite, pokrosvskite
  • step c. a heat-ageing step from 20 to 90°C is performed to obtain complete transformation of dypingite to magnesite after 24 hours.
  • a solid state transition implying the simultaneous dehydration and carbonation of brucitic layer of dypingite precursor coupled with instantaneous formation of magnesite crystals are assumed.
  • the global reaction for dypingite-to-magnesite transformation can be written as follows: 0.2 Mg 5 ( CO 3 ) 4 ( OH ) 2. 5 H 2 O + 0.2 Na 2 CO 3 ⁇ MgCO 3 + 0.4 NaOH + H 2 O (3)
  • the catalytic role can be verified by the reaction balance of reactions 1 to 3.
  • the presence of NaOH also favored the magnesite formation during the heat-ageing step.
  • step b. dypingite is optionally filtered. That means that when dypingite is filtered, step c. must be carried out in an aqueous medium containing a strong base, such as NaOH, KOH, LiOH and RbOH, in particular NaOH, in order to reach a pH higher than 13, in particular 13.5.
  • a strong base such as NaOH, KOH, LiOH and RbOH, in particular NaOH
  • the purity of the obtained magnesite is > 96% based on the thermogravimetric analysis (TGA)
  • the yield or efficiency is close to 1 (or 100%), based in the absence on brucite in the product.
  • the present invention relates to a process of preparation of magnesite and/or hydromagnesite, wherein the CO 2 source in the medium is at an initial pressure comprised from about 40 bar to about 60 bar, in particular 50bar, as defined above, wherein said t 1 time is comprised from 2h to about 4h, in particular 3h, to obtain an intermediate comprising a mixture of residual brucite and a hydrated Mg carbonate in the medium.
  • the introduction of brucite and the strong base is carried out at room temperature and thus an initial temperature (t i ) of about 26°C is observed in the medium before introducing CO 2 , said medium reaching 37 ⁇ 1 °C until the complete or almost complete formation of said intermediate.
  • the present invention relates to a process of preparation of magnesite and/or hydromagnesite, wherein the CO 2 source in the medium is at an initial pressure comprised from about 40 bar to about 60 bar, in particular 50bar, wherein said t 1 time is comprised from 23h to about 25h, in particular 24h, to obtain an intermediate comprising a dypingite precipitate in the medium, as defined above, comprising a further step of heating, after said t 1 time, at a temperature comprised from about 80°C to about 100°C, in particular 90°C, during a t 2 time comprised from about 1h to about 3h, in particular 2h to obtain an hydromagnesite precipitate.
  • the overall synthesis time of hydromagnesite is drastically reduced from 12 days to 5 hours when NaOH is used as catalyst and/or additive in the presence of Mg(OH) 2 -H 2 O-CO 2 . Similar to magnesite synthesis, the NaOH-rich solution accelerates the brucite carbonation by a temporary increase of carbonate ion concentration.
  • the present invention relates to one of the above process of preparation of hydromagnesite comprising the following steps:
  • the hydrothermal carbonation (90°C, 90 bar) of brucite in absence of NaOH forming the hydromagnesite can be illustrated by the following global reaction.
  • the purity of the obtained hydromagnesite is > 96% based on the thermogravimetric analysis (TGA)
  • the yield or efficiency is close to 1 (or 100%), based in the absence on brucite in the product.
  • magnesite and/or hydromagnesite, and/or dypingite of the invention are used as mineral filler and pigment in paper, paint rubber and plastics as well as flame-retardant.
  • the magnesite of the invention can be used as mineral filler in paper and pigments.
  • Hydromagnesite of the invention can be used as a flame-retardant in electric and electronic parts, constructional materials, etc., because their dehydration-dehydroxylation-decarbonation processes consume significant amount of energy in a broad interval of temperature (see Fig. 7 ).
  • platy fine particles and moderate specific surface area (28 m 2 /g) for hydromagnesite can facilitate its dispersion/distribution when it is used as mineral filler or flame-retardant.
  • the carbonation reaction started instantaneously as attested by a continuous consumption of CO 2 (monitored by a pressure drop in the reaction medium) and by an increase of temperature during exothermic carbonation reaction (maximum of temperature ⁇ 38°C after 1h of reaction ( ⁇ T ⁇ 12°C).
  • the autoclave was removed from heating and immersed into cold water.
  • the residual CO 2 was degassed from reactor during water-cooling period.
  • water cooling at 30°C about 15 minutes
  • the autoclave was disassembled, and the solid product was carefully recovered and separated by centrifugation (30 minutes at 12,000 rpm), decanting the supernatant solutions.
  • the solid product was washed twice by re-dispersion/centrifugation processes in order to remove the soluble sodium carbonates formed during the synthesis.
  • the solid product was dried directly in the centrifugation flasks at 80°C for 48 h.
  • the dry solid product was manually recovered, weighed and stored in plastic flasks for further characterizations (FESEM, XRD, TGA and N 2 sorption isotherms).
  • Hydromagnesite-magnesite-brucite composite This composite material was synthesized by a simple modification on the synthesis method for magnesite (see above). More specifically, the carbonation reaction of brucite was carried out in absence of NaOH, leading to the formation of hydromagnesite (dominant phase) and magnesite (minor phase).
  • the final pH is equal to 8.4, measured ex-situ at about 20°C
  • Hydromagnesite-eitelite composite This composite material was synthesized by simple operating modifications on the synthesis method for magnesite (see above). Herein, a heat-ageing step at 45°C was performed immediately after CO 2 injection into the reaction medium.
  • the final pH is equal to 8.4, measured ex-situ at about 20°C
  • the reaction time with Mg(OH) 2 -H 2 O-NaOH-CO 2 was typically 10 days in order to obtain binary hydromagnesite-eitelite composite.
  • the sodium initially contained in NaOH reacts significantly to lead eitelite mineral (Na 2 CO 3 .MgCO 3 ).
  • the NaOH had not only a catalytic affect.
  • the recovery/drying procedures of solid product were the same as described above for magnesite synthesis.
  • FESEM observations magnesite, hydromagnesite and various Mg-carbonate composites from syntheses were dispersed by ultrasonic treatment in absolute ethanol for five to ten minutes. One or two drops of suspension were then deposited directly on an aluminium support for SEM observations, and coated with platinum. Morphological observations of various selected powders were performed using a Zeiss Ultra 55 field emission gun scanning electron microscope (FESEM) that has a maximum spatial resolution of approximately 1nm at 15kV.
  • FESEM Zeiss Ultra 55 field emission gun scanning electron microscope
  • X-Ray Powder Diffraction (XRD) analyses were performed using a D5000, SIEMENS diffractometer in Bragg-Brentano geometry; equipped with a goniometer theta-theta with a rotating sample holder.
  • TGA Thermogravimetric analyses: TGA for all Mg-carbonate samples were performed with a TGA/SDTA 851 e Mettler Toledo instrument under the following conditions: sample mass of about 10 mg, alumina crucible of 150 ⁇ l with a pinhole, heating rate of 5 °C min -1 , and inert N 2 atmosphere of 50 ml min -1 . Sample mass loss and associated thermal effects were obtained by TGA/SDTA. In order to identify the different mass loss steps, the TGA first derivative (rate of mass loss) was used. TGA apparatus was calibrated in terms of mass and temperature. Calcium oxalate was used for the sample mass calibration. The melting points of three compounds (indium, aluminum and copper) obtained from the DTA signals were used for the sample temperature calibration.
  • N 2 sorption isotherms N 2 sorption isotherms for magnesite, hydromagnesite and Mg-carbonate composites were performed by using a sorptomaticTM apparatus (Thermo Electron Corporation). The specific surface area of powdered samples was estimated by applying the Brunauer-Emmet-Teller (BET) equation in the 0.05 ⁇ P/P 0 ⁇ 0.35 interval of relative pressure and by using 16.2 ⁇ 2 for cross-sectional area of molecular N 2 . A non-linear regression by the least-squares method was performed to fit the interval data (n ads vs. P / P 0 ) in the experimental isotherms. Table 1. Summary of experimental conditions for synthesis of anhydrous and hydroxylated Mg-carbonates.
  • BET Brunauer-Emmet-Teller
EP12305943.8A 2012-07-31 2012-07-31 Magnesit- und Hydromagnesit-Herstellungsverfahren Withdrawn EP2692691A1 (de)

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Cited By (2)

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KR20180029867A (ko) 2016-09-12 2018-03-21 주식회사 단석산업 합성 하이드로마그네사이트 입자 및 그의 제조방법
EP3795142A1 (de) 2019-09-12 2021-03-24 FIM Biotech GmbH Poröses magnesiumoxidcarbonat zur verwendung als mittel zur bindung von phosphaten im dünndarm mit dem ziel der reduzierung von nichtübertragbaren krankheiten

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EP2322581A1 (de) 2009-11-03 2011-05-18 Omya Development AG Ausgefälltes Magnesiumcarbonat

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EP3795142A1 (de) 2019-09-12 2021-03-24 FIM Biotech GmbH Poröses magnesiumoxidcarbonat zur verwendung als mittel zur bindung von phosphaten im dünndarm mit dem ziel der reduzierung von nichtübertragbaren krankheiten

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